Method for improving hardness of evaporation coating

Abstract

The invention relates to a method for improving hardness by evaporation coating, which is characterized in that immersion treatment is added between traditional continuous coating of an AR film and an AF film, the binding force and hardness are greatly improved, certain micro-etching treatment is carried out on the surface of glass, and a silicon dioxide auxiliary layer is plated to improve the adhesive force and light transmittance of subsequent coating.

Description

Technical Field

[0001] This invention belongs to the field of coating technology, specifically relating to a method for improving hardness through evaporation coating. Background Technology

[0002] The vapor deposition methods we commonly use result in relatively low surface hardness on glass. Ordinary coating methods cannot even achieve a surface hardness of 2H. Even coating methods using special materials such as ZrO2 and SiO2, heated to over 160℃, can only achieve 5H. As market demands become increasingly stringent, improving the surface hardness of products has become an inevitable direction for the future.

[0003] AR (Arc) film increases light transmittance and improves abrasion resistance by forming a nanoscale optical coating on the glass surface. AF (Abrasion-resistant) film, on the other hand, provides durable anti-fouling capabilities by being layered on top of AR film. However, AR and AF films have different physical and chemical properties, and direct continuous coating may result in insufficient adhesion between the two layers, affecting overall hardness and abrasion resistance. This direct layering method can lead to poor adhesion between the AF and AR films, especially in abrasion tests where the AF film may detach while the AR layer remains undamaged. Therefore, to improve the adhesion and hardness between the two film layers, this invention employs a wet impregnation process to improve the smoothness and condition of the two layers, thereby enhancing bonding strength and hardness.

[0004] Depositing AR films onto glass surfaces offers significant advantages, such as improved optical and mechanical properties, and enhanced surface reflectivity, refractive index, and hardness. However, directly depositing AR films onto glass surfaces presents challenges, including easy detachment and poor adhesion. This is because the films formed during the deposition process are typically porous and have weak bonding strength, leading to easy film detachment. Therefore, although deposition technology can uniformly deposit a layer of material on a surface, the adhesion and stability of the film still require improvements through other processes.

[0005] Research has found that using reverse micelle microemulsions to perform targeted chemical etching on glass, forming spherical pits on the surface that do not affect the appearance of the glass, can increase the contact area between the glass and the film layer, thereby improving the adhesion of the glass surface.

[0006] Interfacial failure easily occurs between glass and organic interlayers due to differences in material properties, which is one of the main factors hindering their widespread application. Studies have found that adding a silica film between inorganic glass and organic interlayers, acting as a performance transition layer, can effectively reduce the performance differences at the inorganic / organic interface. However, the adhesion between the silica film and silicate glass is generally poor, resulting in limited improvement in the overall mechanical properties of the inorganic / organic laminated glass. Therefore, silane coupling agents are often added to couple the interface of two materials with significantly different properties, thereby increasing their interfacial bond strength. However, silane coupling agents can also have varying degrees of impact on the quality of the silica film and the optical properties of the coated glass. This invention aims to improve the quality of the silica film and its impact on the optical properties of the coated glass by selecting an optimal silane coupling agent. Summary of the Invention

[0007] The purpose of this invention is to provide a method for improving hardness through evaporation coating.

[0008] To solve the above-mentioned technical problems, the specific solution of the present invention is as follows: Using a Hall source ion source to assist in the deposition of an AR film, with a deposition chamber temperature of 160℃-200℃, a 50-100nm AR film is deposited on the surface of the glass mold. After deposition and cooling for 1 hour, an AF film is then deposited using a Kaufman ion source, with a deposition temperature of 100℃-160℃ and a thickness of 15-20nm.

[0009] The process of cooling the glass after the AR film is coated also includes an immersion treatment: the immersion solution with a mass fraction of 37% is diluted with ethylene glycol to a 2% immersion ethylene glycol solution, and the cooled glass mold coated with AR film is completely immersed in the diluted solution for 5 minutes. The treated film layer is then cleaned with deionized water and dried in a 120°C drying oven for 1 hour.

[0010] The impregnation solution is composed of N-succinimide solution.

[0011] The glass mold process includes micro-etching: 10-16 parts of emulsifier and 3-5 parts of surfactant are mixed and then mixed with 65-70 parts of n-heptane and 5-10 parts of n-octanol, and stirred for 3 hours to form an oil phase; then, 0.8-1.2 parts of 40% hydrofluoric acid are added at room temperature and stirred for 7 hours to form a clear microemulsion; then, the glass mold is washed with acetone and deionized water and immersed in the microemulsion, and chemically etched at 95°C for 2.5 hours; finally, the chemically etched glass is washed with distilled water and dried to obtain micro-etched glass, and a layer of silica auxiliary film is spin-coated onto the surface of the micro-etched glass.

[0012] The emulsifier is caprylic / capric triglyceride, and the surfactant is hexadecyltrimethylammonium bromide.

[0013] Specifically, the process of spin-coating a silica auxiliary film onto the glass surface after micro-etching involves spin-coating the prepared silica sol onto the glass surface at a spin rate of 3500 r / min for 40 s, followed by drying in a vacuum drying oven at 80 ℃ for 4 h, resulting in a film thickness of 15-20 nm.

[0014] The silica sol is prepared by: adding 1-2 parts of PMHS to 140 parts of anhydrous ethanol and letting it stand at room temperature for 24 hours; then adding 3-4.8% by mass of coupling agent and deionized water, with a PMHS:coupling agent mass ratio of 1:5 and a coupling agent:deionized water mass ratio of 1:4; stirring the mixture vigorously at 600-800 RPM for 3 hours and letting it stand for 24 hours to obtain the silica sol for later use.

[0015] The silane coupling agent is (mentholylethyl)triethoxysilane.

[0016] The beneficial effects of this invention are as follows: 1. The present invention is a method for protecting the glass surface by depositing an AF film layer after the glass surface has been coated with an anti-reflective coating and color-adjusted, and then subjected to a certain impregnation treatment to improve hardness.

[0017] 2. This invention utilizes a reverse micelle microemulsion to perform targeted chemical etching on the glass surface, forming spherical pits that do not affect the glass's appearance. This increases the contact area between the glass and the film layer, disperses vertical forces, and enhances the adhesion strength of subsequent coatings. Furthermore, these pits reduce specular reflection, improving the overall visible light transmittance of the subsequent film layer on the glass mold. In addition, adding a silica transition layer similar to the glass surface further enhances the adhesion between the AR film layer and the glass substrate.

[0018] 3. To improve hardness, a wet immersion process is performed after coating the AR film, followed by coating another AF film. The immersion process improves the properties of the glass surface, making it more suitable for subsequent coating processes. It allows for more thorough exposure of the Si-O atoms on the glass surface, enabling complete reaction between Si atoms and fluorine materials, thereby increasing the adhesion of the film layers. This immersion process not only enhances the adhesion of the AR film but also provides a better foundation for the AF film coating, strengthening the bond between the AF and AR films, thus significantly improving overall hardness and wear resistance.

[0019] 4. The imine group in N-succinimide has a stronger coupling effect with the AR film, which helps the film maintain better mechanical strength under high temperature conditions.

[0020] 5. This invention employs a reverse micelle microemulsion for targeted chemical etching of glass, forming spherical pits on the surface that do not affect the glass's appearance. This increases the contact area between the glass and the film layer and disperses the forces acting in the vertical direction. The molecular structure of caprylic / capric triglycerides contains both hydrophilic and lipophilic groups, enabling it to wet and emulsify within the microemulsion. The hydrophilic groups help disperse the aqueous phase, while the lipophilic groups interact with the oil phase, thus stabilizing the oil-water mixture and forming a microemulsion. This stable microemulsion can effectively perform targeted chemical etching on the glass surface, ensuring the slow release of hydrofluoric acid, thereby forming a micron-sized pit structure on the glass surface. This process not only increases surface roughness but also enhances the adhesion and contact area between the glass and the film layer, strengthens the bonding strength of the film layer, and ultimately improves the optical properties of the glass surface. In the chemically etched reverse micelle microemulsion, the HF encapsulated in the emulsion micelles is slowly released on the contacting glass surface, producing targeted etching and generating dense, micron-sized pits of varying depths on the glass surface, resulting in no visible difference in appearance.

[0021] 6. By etching dense and continuous micron-sized pits on the glass surface using reverse micelle microemulsion etching, not only is the surface roughness of the glass increased, but a wavy 3D film structure is also formed, thereby improving the contact area and adhesion between the film and the glass surface. This structure helps to disperse the force, thereby enhancing the bonding strength of the film. Secondly, the pits generated can reduce specular reflection, which can improve the overall visible light transmittance of subsequent films on the glass surface.

[0022] 7. This invention selects (menthylethyl)triethoxysilane as a coupling agent. The molecule of (menthylethyl)triethoxysilane has a certain degree of amphiphilicity. One end of it is a hydrophobic menthyl group, while the other end is a silane group that can chemically react with inorganic surfaces. This amphiphilic structure allows the molecule to act as a bridge between organic and inorganic materials, improving their interfacial adhesion and compatibility. It has a certain promoting effect on the interfacial adhesion between silica film and inorganic glass. Because the silica sol prepared by (menthylethyl)triethoxysilane has good wettability, it can spread evenly on the glass surface, reducing the phenomenon of large agglomeration of silica film. In addition to increasing interfacial adhesion, (menthylethyl)triethoxysilane, as a coupling agent, can also improve the light transmittance of coated glass.

[0023] 8. By using an appropriate silica ion concentration gradient and transition layer thickness, the adhesion of AR films to glass substrates can be further improved, and the internal stress of AR films on glass can be reduced. Detailed Implementation

[0024] The present invention will be further described in detail below with reference to the embodiments. All glass molds used herein are AGC301, 3mm thick, and purchased from Anyang Iron & Steel Co., Ltd.

[0025] Example 1 Micro-etching process: 13 parts of caprylic / capric triglyceride and 4 parts of hexadecyltrimethylammonium bromide were mixed in a certain proportion, and 68 parts of n-heptane and 8 parts of n-octanol were added and mixed. The mixture was stirred for 3 hours to form an oil phase. Then, 1 part of hydrofluoric acid with a mass fraction of 40% was added to the mixture at room temperature and stirred for 7 hours to form a clear microemulsion. The glass mold was then washed with acetone and deionized water and immersed in the microemulsion. Chemical etching was performed at 95°C for 2.5 hours. Finally, the chemically etched glass was washed with distilled water and dried to obtain the micro-etched glass. A layer of silica auxiliary film was then spin-coated onto the surface of the micro-etched glass.

[0026] Silica sol: 1.5 parts of PMHS were added dropwise to 140 parts of anhydrous ethanol and allowed to stand at room temperature for 24 hours; then 3.9% (mentholylethyl)triethoxysilane and deionized water were added, with the mass ratio of PMHS to (mentholylethyl)triethoxysilane being 1:5 and the mass ratio of (mentholylethyl)triethoxysilane to deionized water being 1:4; the solution was stirred vigorously at 700 RPM for 3 hours and allowed to stand for 24 hours to obtain silica sol for later use.

[0027] A silica auxiliary film was spin-coated onto the micro-etched glass surface: the prepared silica sol was spin-coated onto the glass surface at a spin rate of 3500 r / min for 40 s, and then placed in a vacuum drying oven at 80 ℃ for 4 h. The thickness of the film after formation was 18 nm.

[0028] Using a Hall source ion source to assist in the deposition of an AR film, with the deposition chamber temperature at 180℃, an 80nm AR film is deposited on the surface of the glass mold.

[0029] Example 2 Micro-etching process: 16 parts of caprylic / capric triglyceride and 3 parts of hexadecyltrimethylammonium bromide were mixed in a certain proportion, and 70 parts of n-heptane and 5 parts of n-octanol were added and mixed. The mixture was stirred for 3 hours to form an oil phase. Then, 1.2 parts of hydrofluoric acid with a mass fraction of 40% were added to the mixture at room temperature and stirred for 7 hours to form a clear microemulsion. The glass mold was then washed with acetone and deionized water and immersed in the microemulsion. Chemical etching was performed at 95°C for 2.5 hours. Finally, the chemically etched glass was washed with distilled water and dried to obtain the micro-etched glass. A layer of silica auxiliary film was then spin-coated onto the surface of the micro-etched glass.

[0030] Silica sol: Add 2 parts PMHS to 140 parts anhydrous ethanol and let stand at room temperature for 24 hours; then add 3% (mentholylethyl)triethoxysilane and deionized water, with a mass ratio of PMHS:(mentholylethyl)triethoxysilane of 1:5 and a mass ratio of (mentholylethyl)triethoxysilane:deionized water of 1:4; stir the mixture vigorously at 800 RPM for 3 hours and let stand for 24 hours to obtain silica sol for later use.

[0031] A silica auxiliary film was spin-coated onto the micro-etched glass surface: the prepared silica sol was spin-coated onto the glass surface at a spin rate of 3500 r / min for 40 s, and then placed in a vacuum drying oven at 80 ℃ for 4 h. The thickness of the film after formation was 20 nm.

[0032] Using a Hall source ion source to assist in the deposition of an AR film, with the deposition chamber temperature at 160℃, a 50nm AR film was deposited on the surface of the glass mold.

[0033] Example 3 Micro-etching process: 10 parts of caprylic / capric triglyceride and 5 parts of hexadecyltrimethylammonium bromide were mixed in a certain proportion, and 65 parts of n-heptane and 10 parts of n-octanol were added and mixed. The mixture was stirred for 3 hours to form an oil phase. Then, 0.8 parts of hydrofluoric acid with a mass fraction of 40% were added to the mixture at room temperature and stirred for 7 hours to form a clear microemulsion. The glass mold was then washed with acetone and deionized water and immersed in the microemulsion. Chemical etching was performed at 95°C for 2.5 hours. Finally, the chemically etched glass was washed with distilled water and dried to obtain the micro-etched glass. A layer of silica auxiliary film was then spin-coated onto the surface of the micro-etched glass.

[0034] Silica sol: Add 1 part PMHS to 140 parts anhydrous ethanol and let stand at room temperature for 24 hours; then add 4.8% (mentholylethyl)triethoxysilane and deionized water, with a mass ratio of PMHS:(mentholylethyl)triethoxysilane of 1:5 and a mass ratio of (mentholylethyl)triethoxysilane:deionized water of 1:4; stir the mixture vigorously at 600 RPM for 3 hours and let stand for 24 hours to obtain silica sol for later use.

[0035] A silica auxiliary film was spin-coated onto the micro-etched glass surface: the prepared silica sol was spin-coated onto the glass surface at a spin rate of 3500 r / min for 40 s, and then placed in a vacuum drying oven at 80 ℃ for 4 h. The thickness of the film after formation was 15 nm.

[0036] Using a Hall source ion source to assist in the deposition of an AR film, with a deposition chamber temperature of 200℃, a 100nm AR film is deposited on the surface of a glass mold.

[0037] Comparative Example 1 The difference between this comparative example and Example 1 is that this comparative example does not undergo micro-etching. The specific process is as follows: Silica sol: 1.5 parts of PMHS were added dropwise to 140 parts of anhydrous ethanol and allowed to stand at room temperature for 24 hours; then 3.9% (mentholylethyl)triethoxysilane and deionized water were added, with the mass ratio of PMHS to (mentholylethyl)triethoxysilane being 1:5 and the mass ratio of (mentholylethyl)triethoxysilane to deionized water being 1:4; the solution was stirred vigorously at 700 RPM for 3 hours and allowed to stand for 24 hours to obtain silica sol for later use.

[0038] A silica auxiliary film was spin-coated onto a clean glass surface: the prepared silica sol was spin-coated onto the glass surface at a spin rate of 3500 r / min for 40 s, and then placed in a vacuum drying oven at 80 ℃ for 4 h. The thickness of the film after formation was 18 nm.

[0039] Using a Hall source ion source to assist in the deposition of an AR film, with the deposition chamber temperature at 180℃, an 80nm AR film is deposited on the surface of the glass mold.

[0040] Comparative Example 2 The difference between this comparative example and Example 1 is that the caprylic / capric triglyceride is glyceryl monostearate, while the rest is the same as in Example 1.

[0041] Comparative Example 3 The difference between this comparative example and Example 1 lies in the content of caprylic / capric triglycerides. Specifically, the micro-etching process is as follows: 20 parts of caprylic / capric triglycerides and 4 parts of hexadecyltrimethylammonium bromide are mixed in a specific ratio, and 68 parts of n-heptane and 8 parts of n-octanol are added and mixed. The mixture is stirred for 3 hours to form an oil phase. Then, 1 part of 40% hydrofluoric acid is added at room temperature and stirred for 7 hours to form a clear microemulsion. Next, the glass mold is washed with acetone and deionized water and immersed in the microemulsion for chemical etching at 95°C for 2.5 hours. Finally, the chemically etched glass is washed with distilled water and dried to obtain the micro-etched glass. A layer of silica auxiliary film is then spin-coated onto the surface of the micro-etched glass. The rest is the same as in Example 1.

[0042] Comparative Example 4 The difference between this comparative example and Example 1 lies in the content of caprylic / capric triglycerides. Specifically, the micro-etching process is as follows: 5 parts of caprylic / capric triglycerides and 4 parts of hexadecyltrimethylammonium bromide are mixed in a specific ratio, and 68 parts of n-heptane and 8 parts of n-octanol are added and mixed. The mixture is stirred for 3 hours to form an oil phase. Next, 1 part of 40% hydrofluoric acid is added at room temperature and stirred for 7 hours to form a clear microemulsion. Then, the glass mold is washed with acetone and deionized water and immersed in the microemulsion for chemical etching at 95°C for 2.5 hours. Finally, the chemically etched glass is washed with distilled water and dried to obtain the micro-etched glass. A layer of silica auxiliary film is then spin-coated onto the surface of the micro-etched glass. The rest is the same as in Example 1.

[0043] Comparative Example 5 The difference between this comparative example and Example 1 is that this comparative example does not spin-coat a silicon dioxide auxiliary layer. Specifically: Micro-etching process: 13 parts of caprylic / capric triglyceride and 4 parts of hexadecyltrimethylammonium bromide were mixed in a certain proportion, and 68 parts of n-heptane and 8 parts of n-octanol were added and mixed. The mixture was stirred for 3 hours to form an oil phase. Then, 1 part of hydrofluoric acid with a mass fraction of 40% was added to the mixture at room temperature and stirred for 7 hours to form a clear microemulsion. The glass mold was then washed with acetone and deionized water and immersed in the microemulsion. Chemical etching was performed at 95°C for 2.5 hours. Finally, the chemically etched glass was washed with distilled water and dried to obtain the micro-etched glass.

[0044] Using a Hall source ion source to assist in the deposition of an AR film, with the deposition chamber temperature at 180℃, an 80nm AR film is deposited on the surface of the glass mold.

[0045] Comparative Example 6 The difference between this comparative example and Example 1 is that (mentholylethyl)triethoxysilane is tetraethoxysilane, otherwise it is the same as Example 1.

[0046] Comparative Example 7 The difference between this comparative example and Example 1 lies in the amount of (mentholylethyl)triethoxysilane added. Specifically, the silica sol was prepared as follows: 1.5 parts of PMHS were added dropwise to 140 parts of anhydrous ethanol and allowed to stand at room temperature for 24 hours; then, 3.9% (mentholylethyl)triethoxysilane and deionized water were added, with a PMHS:(mentholylethyl)triethoxysilane mass ratio of 1:3 and a (mentholylethyl)triethoxysilane:deionized water mass ratio of 1:4; the solution was stirred vigorously at 700 RPM for 3 hours and allowed to stand for 24 hours to obtain the silica sol for later use; the rest was the same as in Example 1.

[0047] Comparative Example 8 The difference between this comparative example and Example 1 lies in the amount of (mentholylethyl)triethoxysilane added. Specifically, the silica sol was prepared as follows: 1.5 parts of PMHS were added dropwise to 140 parts of anhydrous ethanol and allowed to stand at room temperature for 24 hours; then, 3.9% (mentholylethyl)triethoxysilane and deionized water were added, with a PMHS:(mentholylethyl)triethoxysilane mass ratio of 1:8 and a (mentholylethyl)triethoxysilane:deionized water mass ratio of 1:4; the solution was stirred vigorously at 700 RPM for 3 hours and allowed to stand for 24 hours to obtain the silica sol for later use; the rest was the same as in Example 1.

[0048] Comparative Example 9 The difference between this comparative example and Example 1 is that micro-etching and spin-coating of silicon dioxide auxiliary layer are not performed in this comparative example. Specifically, an AR film is deposited using a Hall source ion source with a coating chamber temperature of 180°C, and an 80nm AR film is deposited on the surface of the glass mold.

[0049] Experiment 1: The optical properties of the samples prepared in Examples 1-3 and Comparative Examples 1-9 were tested, including the effective transmittance of sunlight and the strength of the glass.

[0050] Effective solar transmittance: The ratio of solar flux transmitted through the sample to incident solar flux within the solar spectrum range of (380 mm ~ 1100 nm).

[0051] Peel strength: The peel strength was measured in accordance with the national standard GB / T 10004-2008.

[0052] The results are shown in Table 1.

[0053] Table 1 The following embodiments are all based on Embodiment 1 with subsequent steps: Example 4 After the glass mold coated with AR film cooled for 1 hour, it was subjected to an immersion treatment. A 37% N-succinimide solution was diluted with ethylene glycol to a 2% immersion ethylene glycol solution. The cooled glass mold coated with AR film was completely immersed in the diluted solution for 5 minutes. The treated film was then cleaned with deionized water and dried in a 120°C drying oven for 1 hour. Then, an AF film was deposited using a Kaufman ion source at a coating temperature of 130°C and a thickness of 18 nm.

[0054] Example 5 After the glass mold coated with AR film cooled for 1 hour, it was subjected to an immersion treatment. A 37% N-succinimide solution was diluted with ethylene glycol to a 2% immersion ethylene glycol solution. The cooled glass mold coated with AR film was completely immersed in the diluted solution for 5 minutes. The treated film was then cleaned with deionized water and dried in a 120°C drying oven for 1 hour. Then, an AF film was deposited using a Kaufman ion source assisted at a coating temperature of 160°C and a thickness of 15 nm.

[0055] Example 6 After the glass mold coated with AR film cooled for 1 hour, it was subjected to immersion treatment. A 37% N-succinimide solution was diluted with ethylene glycol to a 2% immersion ethylene glycol solution. The cooled glass mold coated with AR film was completely immersed in the diluted solution for 5 minutes. The treated film was cleaned with deionized water and dried in a 120℃ drying oven for 1 hour. Then, an AF film was deposited using a Kaufman ion source assisted at a coating temperature of 100℃ and a thickness of 20nm.

[0056] Comparative Example 10 The difference between this comparative example and Example 4 is that no immersion treatment is performed in this comparative example. Specifically, after the glass mold coated with AR film has been cooled for 1 hour, an AF film is deposited using a Kaufman ion source with an assisted coating temperature of 130°C and a thickness of 18 nm.

[0057] Comparative Example 11 The difference between this comparative example and Example 4 is that no cooling treatment is performed after the AR film is deposited in this comparative example. Specifically, the glass mold after the AR film is deposited is immersed in the solution. A 37% N-succinimide solution is diluted with ethylene glycol to a 2% immersion ethylene glycol solution. The glass mold after the AR film is deposited is completely immersed in the diluted solution for 5 minutes. The treated film is then cleaned with deionized water and dried in a 120°C drying oven for 1 hour. Then, an AF film is deposited using a Kaufman ion source assisted at a deposition temperature of 130°C and a thickness of 18 nm.

[0058] Comparative Example 12 The difference between this comparative example and Example 4 is that the N-succinimide in this comparative example is polyethyleneimine, and the rest is the same as in Example 4.

[0059] Comparative Example 13 The difference between this comparative example and Example 4 lies in the amount of N-succinimide added. Specifically, after the glass mold coated with the AR film cooled for 1 hour, it was immersed in the solution. A 37% N-succinimide solution was diluted with ethylene glycol to a 5% immersion ethylene glycol solution. The cooled glass mold coated with the AR film was completely immersed in the diluted solution for 5 minutes. The treated film was then cleaned with deionized water and dried in a 120°C drying oven for 1 hour. Then, an AF film was deposited using a Kaufman ion source at a coating temperature of 130°C and a thickness of 18 nm.

[0060] Comparative Example 14 The difference between this comparative example and Example 4 lies in the amount of N-succinimide added. Specifically, after the glass mold coated with the AR film cooled for 1 hour, it was immersed in the diluted solution. A 37% N-succinimide solution was diluted with ethylene glycol to a 1% immersion ethylene glycol solution. The cooled glass mold coated with the AR film was completely immersed in the diluted solution for 5 minutes. The treated film was then cleaned with deionized water and dried in a 120°C drying oven for 1 hour. Then, an AF film was deposited using a Kaufman ion source at a coating temperature of 130°C and a thickness of 18 nm.

[0061] Experiment 2: Adhesive film adhesion test: According to GB / T9286-2021 Paints and Varnishes - Cross-cut test, based on the sample substrate and adhesive film thickness, the adhesive film is cut into a grid pattern using cross-cutting tools with different spacing, so that it just penetrates to the substrate. The gridded part is then peeled off with 3M tape. The degree of adhesion of the adhesive film is determined by the area of ​​the adhesive film that has fallen off the substrate in the gridded area. The adhesion is divided into 0, 1, 2, 3, 4, 5, 6, 7, 8 and 9 grades, with grade 9 being the best and grade 0 being the worst.

[0062] Hardness test: The hardness of the coating film was measured using a pencil scratch hardness tester according to GB / T6739-2022 "Determination of Hardness of Coating Film by Pencil Method".

[0063] The results are shown in Table 2 below.

[0064] Table 2

Claims

1. A method for improving hardness through evaporation coating, characterized in that: Using Hall source ion source to assist in AR film deposition, the deposition chamber temperature is 160℃-200℃, and a 50-100nm AR film is deposited on the surface of the glass mold. After deposition, the mold is cooled for 1 hour and then Kaufman ion source is used to assist in AF film deposition, with a deposition temperature of 100℃-160℃ and a thickness of 15-20nm. When the glass is cooled after being coated with AR film, it also includes an immersion treatment: the immersion solution with a mass fraction of 37% is diluted with ethylene glycol to a 2% immersion ethylene glycol solution, and the glass mold after being coated with AR film and cooled is completely immersed in the diluted solution for 5 minutes. The treated film layer is cleaned with deionized water and dried in a drying oven at 120°C for 1 hour.

2. The method for improving hardness through evaporation coating as described in claim 1, characterized in that: The impregnation solution is an N-succinimide solution.

3. The method for improving hardness through evaporation coating as described in claim 1, characterized in that: The glass mold also includes a micro-etching process: 10-16 parts of emulsifier and 3-5 parts of surfactant are mixed, and then mixed with 65-70 parts of n-heptane and 5-10 parts of n-octanol, and stirred for 3 hours to form an oil phase; then, 0.8-1.2 parts of hydrofluoric acid with a mass fraction of 40% are added to it at room temperature, and stirred for 7 hours to form a clear microemulsion; then, the glass mold is washed with acetone and deionized water and immersed in the microemulsion, and chemically etched at 95°C for 2.5 hours; finally, the chemically etched glass is washed with distilled water and dried to obtain micro-etched glass, and a layer of silica auxiliary film is spin-coated on the surface of the micro-etched glass.

4. The method for improving hardness through evaporation coating as described in claim 3, characterized in that: The emulsifier is caprylic / capric triglyceride, and the surfactant is hexadecyltrimethylammonium bromide.

5. The method for improving hardness through evaporation coating as described in claim 3, characterized in that: The process of spin-coating a silica auxiliary film onto the micro-etched glass surface involves spin-coating the prepared silica sol onto the glass surface at a spin rate of 3500 r / min for 40 s, followed by drying in a vacuum drying oven at 80°C for 4 h. The resulting film has a thickness of 15-20 nm.

6. The method for improving hardness through evaporation coating as described in claim 5, characterized in that: The silica sol is prepared by: adding 1-2 parts of PMHS to 140 parts of anhydrous ethanol and letting it stand at room temperature for 24 hours; then adding 3-4.8% by mass of coupling agent and deionized water, with the mass ratio of PMHS to coupling agent being 1:5 and the mass ratio of coupling agent to deionized water being 1:4; stirring the mixture vigorously at 600-800 RPM for 3 hours and letting it stand for 24 hours to obtain the silica sol for later use.

7. The method for improving hardness through evaporation coating as described in claim 6, characterized in that: The coupling agent is (mentholylethyl)triethoxysilane.

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